CN108499742B - Application of phenylpropenyl hydroximic acid in flotation of ilmenite and bastnaesite - Google Patents

Application of phenylpropenyl hydroximic acid in flotation of ilmenite and bastnaesite Download PDF

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CN108499742B
CN108499742B CN201810249255.XA CN201810249255A CN108499742B CN 108499742 B CN108499742 B CN 108499742B CN 201810249255 A CN201810249255 A CN 201810249255A CN 108499742 B CN108499742 B CN 108499742B
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hydroximic acid
flotation
phenyl
acid
ilmenite
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CN108499742A (en
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余新阳
王礼平
胡琳琪
王浩林
王强强
黄志强
何桂春
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Jiangxi University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/01—Organic compounds containing nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B1/00—Conditioning for facilitating separation by altering physical properties of the matter to be treated
    • B03B1/04—Conditioning for facilitating separation by altering physical properties of the matter to be treated by additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/007—Modifying reagents for adjusting pH or conductivity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/02—Collectors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; specified applications
    • B03D2203/02—Ores
    • B03D2203/04—Non-sulfide ores

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Abstract

The invention relates to the field of flotation, in particular to application of phenylpropenyl hydroximic acid in flotation of ilmenite and bastnaesite. The invention is applied to the flotation of ilmenite or bastnaesite, and the flotation process conditions are as follows: the dosage of the collecting agent phenylpropenyl hydroximic acid is more than or equal to 15g/t, the ore granularity is minus 0.074mm and accounts for 60-100%, lime, sodium hydroxide or sodium carbonate are added to adjust the pH value of ore pulp to 4-12, water glass is used as an inhibitor and the dosage is 200-2000 g/t, MIBC is used as a foaming agent and the dosage is 10-20 mg/L, and the action time is about 1 min. The invention is easy to operate, reduces the burden of workers, saves medicaments and reduces the beneficiation cost.

Description

Application of phenylpropenyl hydroximic acid in flotation of ilmenite and bastnaesite
Technical Field
The invention relates to the field of flotation, in particular to application of phenylpropenyl hydroximic acid in flotation of ilmenite and bastnaesite.
Background
Rare earth metals are called "vitamins" and are widely used in the fields of energy, aerospace, military, information, electronics, machinery, and the like. At present, the global rare earth resources mainly come from bastnaesite, monazite and ion adsorption type rare earth ore in south China. The reserves and the yields of rare earth resources in China are listed as the first world, and the rare earth resources in China are the mainIs present in bastnaesite. The rare earth beneficiation technology in China achieves certain achievement after decades of research and development, but still has some problems and defects, such as low resource recovery rate, high processing cost, poor concentrate quality and the like. Flotation is one of the main beneficiation methods of rare earth minerals, and is particularly directed at micro-fine particle refractory rare earth minerals. Hydroximic acid is a chelating collector with excellent performance and is widely applied to the flotation process of rare earth ores such as bastnaesite, ilmenite, tantalum-niobium ore and the like. It is believed that the hydroxamic acids or their alkali metal salts can react with Cu2+、Fe3+Generating chelate by plasma to generate 0, and adsorbing the O five-membered ring complex on the surface of the mineral to enhance the hydrophobicity of the surface of the mineral. The hydroximic acid currently applied to the rare earth ore flotation collector mainly comprises alkyl hydroximic acid, salicylaldoxime, salicylhydroxamic acid, naphthyl hydroximic acid, N-hydroxyphthalimide and the like, wherein the salicylhydroxamic acid is most widely applied. Flotation practices show that the collecting agent applied to industrial production not only requires stronger collecting capacity and good selectivity, but also has the advantages of environmental friendliness, low price, wide source and good operability. At present, most of collecting agents for rare earth mineral flotation have the problems and disadvantages of sensitivity to slime, weak collecting capability, poor selectivity, high medicament cost and the like, and the application and popularization of the rare earth flotation technology are severely restricted. Therefore, the research on the novel and efficient rare earth mineral flotation collector has important practical value for improving the comprehensive utilization rate of rare earth resources in China and relieving the pressure of the rare earth resources.
Disclosure of Invention
The invention aims to provide application of phenyl-propenyl hydroximic acid in flotation of ilmenite and bastnaesite.
The technical scheme of the invention is as follows:
the phenylpropenyl hydroximic acid is used as a collecting agent and applied to flotation of ilmenite and bastnaesite, the pH value of ore pulp in the flotation is 4-12, and the molecular formula of the phenylpropenyl hydroximic acid is C9H9NO2The molecular structure is shown as formula-I,
Figure BDA0001607374770000011
a flotation method of ilmenite or bastnaesite comprises the following flotation process conditions: the dosage of the collecting agent phenylpropenyl hydroximic acid is more than or equal to 15g/t (namely more than or equal to 5mg/L), the ore granularity is-0.074 mm and accounts for 60-100%, hydrochloric acid, lime, sodium hydroxide or sodium carbonate is added to adjust the pH of ore pulp to be 4-12, water glass is an inhibitor, the dosage is 200-2000 g/t, MIBC is a foaming agent, the dosage is 10-20 mg/L, and the action time is about 1 min.
The phenyl vinyl hydroximic acid collecting agent used in the invention has strong collecting capacity on oxide ores such as ilmenite, fluorocarbon cerium and the like, the pH range of the suitable flotation pulp is 4-11, and the using amount is more than or equal to 15g/t (equivalent to more than or equal to 5 mg/L). The structure of the phenyl propenyl hydroximic acid is shown as the formula-I, the molecular structure of the phenyl propenyl hydroximic acid contains a benzene ring and a carbon-carbon double bond, and the alkenyl of the phenyl propenyl hydroximic acid, the benzene ring and the hydroximic group form a large conjugated structure, so that the electron cloud of the phenyl propenyl hydroximic acid is denser, the nucleophilicity of the phenyl propenyl hydroximic acid and metal ions is stronger, the phenyl propenyl hydroximic acid and the hydroximic acid are more prone to generating a chelating coordination reaction with the metal ions than the hydroximic acid without the conjugated structure, and the collecting capacity is stronger; the double bonds are contained in the molecules, so that the mineral water has a lower freezing point, has good dispersibility in mineral slurry, and is more suitable for being used under low-temperature conditions. The optimum pH value of the phenylpropyl hydroximic acid in the ore pulp is close to neutral, the operation is easy, the burden of workers is reduced, the medicament is saved, and the ore dressing cost is reduced.
Drawings
Fig. 1 is a flow chart of an experiment for flotation of bastnaesite or ilmenite monomineral by using a phenyl propenyl hydroximic acid collector and other hydroximic acid collectors used in the present invention.
Figure 2 is a flow diagram of a small closed circuit test for the flotation of a rare earth gravity concentrate using a phenylpropenyl hydroximic acid collector in accordance with the present invention (example 4).
Detailed Description
The phenylpropenyl hydroximic acid collecting agent used by the invention is prepared by the following steps:
(1) preparing raw materials, namely taking methyl phenylacrylate, hydroxylamine hydrochloride and sodium hydroxide as raw materials, wherein the molar ratio of the methyl phenylacrylate to the hydroxylamine hydrochloride to the sodium hydroxide is 1.0: 1.1-1.5: 2.2-3.0;
(2) preparing hydroxylamine hydrochloride and a solution needing sodium hydroxide, dissolving the hydroxylamine hydrochloride in distilled water, magnetically stirring at a stirring speed of 500 r/min-1000 r/min, heating in an oil bath at a constant temperature of 30 ℃, adding 3 batches of the needed sodium hydroxide in 30min, and then fully dissociating;
(3) preparing a crude product of the phenyl-propenyl hydroximic acid, adding methyl phenylacrylate with a structure shown in a formula-II into the solution obtained in the step (2), heating the mixture in an oil bath at a constant temperature of 45-60 ℃ for 3-5 h, and acidifying the obtained reaction solution by using sulfuric acid after the reaction is finished to obtain the crude product of the phenyl-propenyl hydroximic acid;
Figure BDA0001607374770000031
(4) and (3) purifying the phenyl hydroxyl hydroximic acid, dissolving the phenyl hydroxyl hydroximic acid crude product obtained in the step (3) with hot water, cooling to room temperature, filtering, repeatedly dissolving the filtered precipitate with hot water, cooling, and filtering for 2-3 times to obtain the high-purity phenyl hydroxyl hydroximic acid.
The invention is further illustrated by, but is not limited to, the following examples. All amounts and percentages in the examples refer to quality parameters unless otherwise indicated.
When the phenyl propenyl hydroximic acid is applied to the ore flotation collector, the main operation flow is as follows: grinding the selected ore to the required floatation granularity, then adding a regulator, a collecting agent phenylpropenyl hydroximic acid and a foaming agent, and then re-aerating, floating and scraping bubbles to obtain the useful metal mineral.
Example 1: preparation of phenyl propenyl hydroximic acid
Pouring 90mL of distilled water into a 500mL three-neck flask, heating by an oil bath at the constant temperature of 30 ℃, and condensing and refluxing at normal temperature; firstly, adding 8.34 parts of hydroxylamine hydrochloride into a three-neck flask, then adding 8.8 parts of sodium hydroxide in batches, and reacting for 30 min; fully dissociating hydroxylamine; adding methyl phenylacrylate with a structure shown in formula-II into the free solution, heating the reaction system in a constant-temperature oil bath at 50 ℃ for 4h, and after the reaction is finished, acidifying the obtained reaction solution by using sulfuric acid to obtain a crude phenylalkenyl hydroximic acid product; and dissolving the crude product in hot water, cooling, filtering, and repeatedly purifying for 2-3 times to obtain the high-purity phenylpropenyl hydroximic acid. The reaction process is shown as the formula-III.
Figure BDA0001607374770000032
Example 2 comparison of flotation Performance of Phenylhydroxamic acid collectors to other hydroximic acid collectors on Fluorocerous Monominerals
The ore feeding granularity of the fluorine-carbon-cerium single mineral is 0.074 mm-0.038 mm. Firstly, adding 2g of pure minerals and 35mL of distilled water into a flotation tank, and stirring and mixing the slurry for 1 min; then adjusting the pH value of the ore pulp to a set value by using hydrochloric acid or NaOH, and stirring for 2 min; then, adding a collecting agent hydroximic acid in sequence, reacting for 3min, a foaming agent MIBC15mg/L, reacting for 1min, and finally aerating and scraping for 5 min; and after the flotation test is finished, filtering, drying and weighing the foam product, and calculating the recovery rate. The detailed test procedure and drug regimen are shown in FIG. 1, and the test results are shown in tables 1 and 2.
TABLE 1 results of research on flotation performance test of hydroximic acid on fluorocarbon cerium monomineral (%)
Figure BDA0001607374770000041
TABLE 2 result of research on flotation performance test of the amount of phenylpropenyl hydroximic acid to fluorocarbon cerium monomineral (%)
Figure BDA0001607374770000042
Example 3 comparison of Phenylphenylhydroxamic acid collectors with other hydroximic acid collectors for flotation of ilmenite Mono minerals
The feeding granularity of the ilmenite is 0.074 mm-0.038 mm. Firstly, adding 2g of pure minerals and 35mL of distilled water into a flotation tank, and stirring and mixing for 1 min; then adjusting the pH value of the ore pulp to the setting values shown in the table 7 and the table 8 by using hydrochloric acid or NaOH, and stirring for 2 min; then, adding hydroximic acid serving as a collecting agent into the mixture in sequence, reacting for 3min, adding a foaming agent MIBC15mg/L, reacting for 1min, and finally aerating and scraping for 5 min; and after the flotation test is finished, filtering, drying and weighing the foam product, and calculating the recovery rate. The detailed test procedure and drug regimen are shown in FIG. 1, and the test results are shown in tables 3 and 4.
TABLE 3 results of research on flotation performance test of hydroximic acid on ilmenite pure mineral (%)
Figure BDA0001607374770000043
TABLE 4 results of experimental investigation of flotation properties of pure ilmenite using amount of phenylpropenyl hydroxamic acid (%)
Figure BDA0001607374770000044
Example 4: reselection rough concentrate of rare earth from phenylpropyl hydroximic acid flotation Sichuan
In this example, the test sample is obtained from crude ore concentrate produced by gravity separation of rare earth from Sichuan, the REO content of the test sample is 12.87%, the rare earth minerals mainly include bastnaesite and monazite, and the gangue minerals mainly include barite, quartz, feldspar, mica, spodumene, fluorite, iron minerals, etc. The small closed circuit test procedure and the dosage regime are shown in FIG. 2, and the results are shown in Table 5.
TABLE 5 results of a small closed circuit test for flotation of a rare earth ore in Sichuan (%)
Figure BDA0001607374770000051

Claims (1)

1. An application of phenyl propenyl hydroximic acid in ilmenite flotation is characterized in that the molecular structure of the phenyl propenyl hydroximic acid is shown in the formula-I,
Figure FDF0000016351380000011
the preparation method of the phenylpropenyl hydroximic acid comprises the following steps:
(1) preparing raw materials, namely taking methyl phenylacrylate, hydroxylamine hydrochloride and sodium hydroxide as raw materials, wherein the molar ratio of the methyl phenylacrylate to the hydroxylamine hydrochloride to the sodium hydroxide is 1.0: 1.1-1.5: 2.2-3.0;
(2) preparing hydroxylamine hydrochloride and a solution needing sodium hydroxide, dissolving the hydroxylamine hydrochloride in distilled water, magnetically stirring at a stirring speed of 500 r/min-1000 r/min, heating in an oil bath at a constant temperature of 30 ℃, adding 3 batches of the needed sodium hydroxide in 30min, and then fully dissociating;
(3) preparing a crude product of the phenyl-propenyl hydroximic acid, adding methyl phenylacrylate with a structure shown in a formula-II into the solution obtained in the step (2), heating the mixture in an oil bath at a constant temperature of 45-60 ℃ for 3-5 h, and acidifying the obtained reaction solution by using sulfuric acid after the reaction is finished to obtain the crude product of the phenyl-propenyl hydroximic acid;
Figure FDF0000016351380000012
(4) purifying the phenyl hydroximic acid, dissolving the phenyl hydroximic acid crude product obtained in the step (3) with hot water, cooling to room temperature, filtering, repeatedly dissolving the precipitate obtained by filtering with hot water, cooling, and filtering for 2-3 times to obtain the phenyl hydroximic acid;
the flotation step comprises: feeding ilmenite with the granularity of 0.074 mm-0.038 mm, adding 2g of pure mineral and 35mL of distilled water into a flotation tank, and stirring and mixing for 1 min; then adjusting the pH value of the ore pulp to 6-9 by using hydrochloric acid or NaOH, and stirring for 2 min; then, adding a collecting agent phenylpropyl alkenyl hydroximic acid in sequence, reacting for 3min, a foaming agent MIBC15mg/L, reacting for 1min, and finally aerating and scraping for 5 min; after the flotation test is finished, filtering, drying and weighing the foam product, and calculating the recovery rate; wherein the dosage of the phenyl vinyl hydroximic acid is 40-80 mg/L.
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CN109772592B (en) * 2019-03-13 2021-03-23 广东省科学院资源综合利用研究所 Application of 2-hydroxy aronoxime compound as collecting agent in oxide ore flotation and flotation method
CN109913648B (en) * 2019-03-13 2021-07-09 广东省资源综合利用研究所 Application of 2-hydroxy aronoxime compound as extracting agent in extraction field, composite extracting agent and extraction system
CN110449256A (en) * 2019-07-31 2019-11-15 中国恩菲工程技术有限公司 The beneficiation method of bastnaesite
CN110449257B (en) * 2019-07-31 2021-12-07 中国恩菲工程技术有限公司 Beneficiation method of bastnaesite
CN110813541B (en) * 2019-10-24 2021-05-28 商洛学院 Collector combination for flotation of monazite and xenotime from fine-grained seashore placer

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